CN102909383A - Method for preparing ultrafine nickel powder or cobalt powder - Google Patents
Method for preparing ultrafine nickel powder or cobalt powder Download PDFInfo
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- CN102909383A CN102909383A CN2011102214092A CN201110221409A CN102909383A CN 102909383 A CN102909383 A CN 102909383A CN 2011102214092 A CN2011102214092 A CN 2011102214092A CN 201110221409 A CN201110221409 A CN 201110221409A CN 102909383 A CN102909383 A CN 102909383A
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Abstract
The invention is applicable to the field of preparation of metal particles, and provides a method for preparing ultrafine nickel powder or cobalt powder. The method includes ball-milling, primary airflow crushing and classification treatment, reduction treatment, and secondary airflow crushing and classification treatment. The method for preparing the ultrafine nickel powder or cobalt powder has the advantages that ball-milling and airflow crushing are combined, so that hard aggregates and soft aggregates in nickel powder precursors or cobalt powder precursors are crushed and scattered, re-aggregation of the nickel powder precursors or cobalt powder precursors is effectively prevented after the nickel powder precursors or cobalt powder precursors are subjected to ball-milling, the secondary airflow crushing is carried out after the reduction treatment, so that the aggregates in nickel powder or cobalt powder are crushed and scattered again, aggregation of the nickel powder or cobalt powder is effectively prevented after the nickel powder or cobalt powder is subjected to the reduction treatment, and the particle size of the ultrafine nickel powder or cobalt powder is uniform. Besides, operation is simple, cost is low, and the method is quite suitable for industrial production.
Description
Technical field
The invention belongs to the metal particle preparing technical field, relate in particular to the preparation method of a kind of extra-fine nickel powder or cobalt powder.
Background technology
At present, it is raw material that the preparation super-fine cobalt powder adopts cobalt carbonate or cobalt oxalate, add a certain proportion of dispersant, under the argon shield environment through the vacuum ball milling, and in hydrogen atmosphere, reduce and make, but this method need to vacuumize ball grinder, and need to lead to argon shield, Ball-milling Time is long, so production cost is higher; Simultaneously, the nickel powder of prepared production or the particle size of cobalt powder differ, and be inhomogeneous, can't meet the needs of production.
Summary of the invention
In view of this, the embodiment of the invention provides the preparation method of a kind of extra-fine nickel powder or cobalt powder, solves in the prior art preparation extra-fine nickel powder or the cobalt powder cost is high, nickel powder or the inhomogeneous technical problem of cobalt powder particle diameter.
The present invention is achieved in that
The preparation method of a kind of extra-fine nickel powder or cobalt powder comprises the steps:
With powdered nickel precursor body or cobalt powder presoma ball milling 3-20 hour;
Powdered nickel precursor body behind the ball milling or cobalt powder presoma are carried out airflow crash, classification processing, by broken and classifying turbine frequency, collect powdered nickel precursor body or the cobalt powder presoma of target grain size;
Be calcination process under the 300-450 ℃ of condition with this powdered nickel precursor body or cobalt powder presoma at reducing atmosphere and temperature, obtain nickel powder or cobalt powder;
This nickel powder or cobalt powder are carried out airflow crash, classification processing, by broken and classifying turbine frequency, obtain extra-fine nickel powder or cobalt powder.
The extra-fine nickel powder of the embodiment of the invention or the preparation method of cobalt powder, by ball milling and airflow crash are combined with, so that hard agglomeration and soft aggregate in powdered nickel precursor body or the cobalt powder presoma all be broken, disperse, powdered nickel precursor body behind the ball milling or the again reunion of cobalt powder presoma have effectively been prevented; Carry out again airflow crash after processing by reduction, so that the soft aggregate in nickel powder or the cobalt powder obtains again broken the dispersion, effectively prevented nickel powder after reduction is processed or the reunion of cobalt powder, realized the uniform particle diameter of extra-fine nickel powder or cobalt powder.The preparation method of the embodiment of the invention, simple to operate, with low cost, be very suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the preparation method's of embodiment of the invention extra-fine nickel powder or cobalt powder flow chart;
Fig. 2 is the preparation method's of the embodiment of the invention one extra-fine nickel powder or cobalt powder flow chart;
Fig. 3 is the prepared super-fine cobalt powder electron microscope photo scanning of the embodiment of the invention three.
The specific embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
See also Fig. 1, Fig. 1 shows the preparation method's of a kind of extra-fine nickel powder of the embodiment of the invention or cobalt powder flow chart, comprises the steps:
Step S01, ball milling
With powdered nickel precursor body or cobalt powder presoma ball milling 3-20 hour;
Step S02, for the first time airflow crash, classification processed
Powdered nickel precursor body behind the ball milling or cobalt powder presoma are carried out airflow crash, classification processing, collect nickel powder forerunner or cobalt powder presoma;
Step S03, reduction
Be calcination process under the 300-450 ℃ of condition with this nickel powder precursor or cobalt powder precursor at reducing atmosphere and temperature, obtain nickel powder or cobalt powder;
Step S04, for the second time airflow crash, classification processed
This nickel powder or cobalt powder are carried out airflow crash, classification processing, collect nickel powder or cobalt powder, obtain extra-fine nickel powder or cobalt powder.
Particularly, this powdered nickel precursor body is selected from one or more in nickelous carbonate, nickel oxalate, nickel oxide, nickel protoxide or the nickel hydroxide; This cobalt powder precursor is selected from one or more in cobalt carbonate, cobalt oxalate, cobalt oxide, cobalt protoxide or the cobalt hydroxide.
Particularly, among the step S01, the employed equipment of this ball milling is restriction not, for example, and planetary power ball mill, high-energy stirring ball mill machine etc.; Ball-milling Time is 3-20 hour, is preferably 10-20 hour; In the ball milling step, the rotating speed of ball-grinding machine is 100-300 rev/min.By ball-milling treatment, powdered nickel precursor body or cobalt powder presoma are carried out the fragmentation dispersion, particularly to some hard agglomerations in the nickel cobalt powder presoma, played effective especially broken peptizaiton.
Particularly, among the step S02, this airflow crash, classification are processed and are referred to, through fragmentation, the screening of the broken grader of hypersonic air flow, obtain the powder of target grain size.To process employed equipment be fluidized bed air flow crusher for airflow crash, classification in this step, fluidized bed air flow crusher is a kind of equipment of realizing the dry type material superfine comminution with high velocity air, it forms by pulverizing nozzle, grading rotor, screw feeder etc., material enters pulverizing chamber by screw feeder, press fast air to pass through the superonic flow nozzzle of particular arrangement to the pulverizing chamber high velocity jet, material accelerates in the superonic flow nozzzle jet, and in the repeated stock of nozzle intersection, collision, reach pulverizing.Entered grading room by comminuting matter with ascending air, because classification turns from High Rotation Speed, particle both had been subject to the centrifugal force that grading rotor produces, be subject to again the centripetal force that the air-flow viscous effect produces, when particle is subject to centrifugal force greater than centripetal force, be that the above corase particles in classification footpath returns pulverizing chamber and continues impact comminution, the following fine particle in classification footpath with air-flow enter cyclone separator, trap is collected, gas is discharged by air-introduced machine.In the airflow crash step, the frequency of the broken grader of this hypersonic air flow is that 30-70HZ/ divides; The atmosphere of this airflow crash is restriction not, such as air, inert atmosphere (such as nitrogen atmosphere, argon gas atmosphere etc.), and reducing atmosphere (hydrogen atmosphere, carbon monoxide atmosphere etc.) etc.Because the mechanical milling process of step S01 can produce a large amount of heat, make the moisture evaporation in powdered nickel precursor body or the cobalt powder presoma, form water vapour, simultaneously in the mechanical milling process because of powder fining, surface energy increases, and powder easily forms aggregate again, after the airflow crash of step S02 is processed, can effectively this aggregate be disperseed, so that powdered nickel precursor body or cobalt powder presoma obtain effective fragmentation; The particle diameter of the powdered nickel precursor body that this step S02 obtains or cobalt powder presoma is more than 200 orders.
Among this step S02, the broken grader of hypersonic air flow comes controlled fragmentation and grading effect by broken frequency, is separated after powder diameter reaches requirement, and the end reaches the particle diameter requirement and returns crusher chamber continuation fragmentation, collects target powder, enters in next step processing;
Particularly, among the step S03, the powdered nickel precursor body collected among the step S02 or cobalt powder presoma are reduced processing, the temperature that reduction is processed is 300-450 ℃, is preferably 360-420 ℃; The time that reduction is processed is 2-6 hour; This reducing atmosphere is restriction not, formed by reducibility gas and inert gas, this reducibility gas for example, hydrogen, carbon monoxide; This inert atmosphere for example, nitrogen, helium, argon gas etc.; In this reducing atmosphere, the volume ratio of reducibility gas and inert gas is 1: 0.1-2.5.Reduction through this step is processed, and makes powdered nickel precursor body or the cobalt powder presoma collected among the step S02 be reduced into nickel powder or cobalt powder.
Particularly, among the step S04, the broken classification of this hypersonic air flow is processed identical with aforesaid principle, does not repeat to set forth at this.Wherein, among this step S04, the atmosphere of airflow crash is inert atmosphere, and this inert atmosphere does not repeat to set forth at this with aforesaid identical; The frequency of the broken grader of this hypersonic air flow is that 30-70HZ/ divides.Because the reduction of step S03 can produce water vapour in processing, so that the nickel powder in this step or cobalt powder are grown up and again reunion, so that prepared nickel powder or cobalt powder particle size differ, do not have uniformity, can not meet the needs of production; Preparation-obtained nickel powder or cobalt powder disperse so that the aggregate in nickel powder or the cobalt powder carries out fragmentation through the broken classification processing of the hypersonic air flow of step S04 among the step S03; By adjusting broken frequency, obtain that particle diameter is little, narrowly distributing extra-fine nickel powder or cobalt powder.Process through step S04, the Fei Shi particle diameter of resulting extra-fine nickel powder or cobalt powder is the FSSS0.5-1.0 micron, and oxygen content is 0.4-0.8%.
The extra-fine nickel powder of the embodiment of the invention or the preparation method of cobalt powder, by ball milling and airflow crash are combined with, so that hard agglomeration and soft aggregate in powdered nickel precursor body or the cobalt powder presoma all be broken, disperse, powdered nickel precursor body behind the ball milling or the again reunion of cobalt powder presoma have effectively been prevented; Carry out again airflow crash after processing by reduction, so that the soft aggregate in nickel powder or the cobalt powder obtains again broken the dispersion, effectively prevented nickel powder after reduction is processed or the again reunion of cobalt powder, realized the uniform particle diameter of extra-fine nickel powder or cobalt powder.
Preparation method to above-mentioned extra-fine nickel powder or cobalt powder is described in detail below in conjunction with specific embodiment.
Embodiment one
See also Fig. 2, Fig. 2 shows the embodiment of the invention one super-fine cobalt powder preparation method idiographic flow, comprises the steps:
Be ball milling 10 hours under 100 rev/mins of conditions with cobalt carbonate at rotating speed;
Cobalt carbonate behind the ball milling is carried out airflow crash, classification processing, and broken frequency is 45HZ, obtains cobalt powder presoma ultrafine particle powder;
It is calcination process under 380 ℃ of conditions at nitrogen and hydrogen (nitrogen with hydrogen volume than 2.5: 1) and temperature that body before this cobalt powder is driven the body powder, obtains cobalt powder;
This cobalt powder is carried out airflow crash, classification processing, and the airflow crash frequency is 40HZ, obtains super-fine cobalt powder, cobalt powder FSSS0.75um, oxygen 0.55%.
Embodiment two
Embodiment of the invention extra-fine nickel powder preparation method comprises the steps:
Be ball milling 10 hours under 200 rev/mins of conditions with nickel oxalate at rotating speed;
Nickelous carbonate behind the ball milling is carried out airflow crash, classification processing, and broken frequency is that 50HZ obtains powdered nickel precursor body.Be calcination process under 370 ℃ of conditions with this powdered nickel precursor body at carbon monoxide and nitrogen mixture body (carbon monoxide and nitrogen volume ratio 1: 0.1) and temperature, obtain nickel powder;
This nickel powder or nickel powder are carried out airflow crash, classification processing, and the airflow crash frequency is that 30HZ obtains extra-fine nickel powder, nickel powder FSSS0.65um, oxygen content 0.61%.
Embodiment three
Embodiment of the invention super-fine cobalt powder preparation method comprises the steps:
Be ball milling 20 hours under 300 rev/mins of conditions with cobalt hydroxide at rotating speed;
Cobalt hydroxide behind the ball milling is carried out airflow crash, classification processing, and broken frequency is that 70HZ obtains the cobalt powder presoma.Be calcination process under 450 ℃ of conditions with this cobalt powder presoma at hydrogen and nitrogen mixture body (hydrogen and nitrogen volume ratio 1: 1.25) and temperature, obtain cobalt powder;
This cobalt powder is carried out airflow crash, classification processing, and the airflow crash frequency is that 40HZ obtains super-fine cobalt powder.Cobalt powder FSSS0.55um, oxygen content 0.65%.See also Fig. 3, Fig. 3 shows the super-fine cobalt powder electron microscope photo scanning that the embodiment of the invention three is prepared, and as can be seen from Figure 3, this cobalt powder particle diameter is little and even.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of an extra-fine nickel powder or cobalt powder comprises the steps:
With nickel powder precursor or cobalt powder precursor ball milling 3-20 hour;
Powdered nickel precursor body behind the ball milling or cobalt powder presoma are carried out airflow crash, classification processing, collect powdered nickel precursor body or cobalt powder presoma;
Be calcination process under the 300-450 ℃ of condition with described powdered nickel precursor body or cobalt powder presoma at reducing atmosphere and temperature, obtain nickel powder or cobalt powder;
Described nickel powder or cobalt powder are carried out airflow crash, classification processing, collect extra-fine nickel powder or cobalt powder.
2. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, described powdered nickel precursor body is selected from one or more in nickelous carbonate, nickel oxalate, nickel oxide, nickel protoxide or the nickel hydroxide; Described cobalt powder presoma is selected from one or more in cobalt carbonate, cobalt oxalate, cobalt oxide, cobalt protoxide or the cobalt hydroxide.
3. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, the rotating speed during described ball milling is 100-300 rev/min.
4. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, the time of described ball milling is 10-20 hour.
5. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, described milling atmosphere is air atmosphere.
6. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, the frequency of described air current classifying fragmentation is that 30-70HZ/ divides.
7. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, described reducing atmosphere is the mixed atmosphere that reducibility gas and inert gas form.
8. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, the time of described calcination process is 2-6 hour.
9. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, described nickel powder or cobalt powder are carried out in airflow crash, the classification treatment step, and the atmosphere of airflow crash is inert atmosphere.
10. the preparation method of extra-fine nickel powder as claimed in claim 1 or cobalt powder is characterized in that, described nickel powder or cobalt powder oxygen content are 0.4-0.8%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104646679A (en) * | 2013-11-19 | 2015-05-27 | 荆门市格林美新材料有限公司 | Method for manufacturing spherical Fe-Co-Ni alloy powder |
| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN104942301A (en) * | 2015-06-19 | 2015-09-30 | 四川金广实业（集团）股份有限公司 | Technology for producing nickel raw material for stainless steel by nickelous hydroxide |
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN106799498A (en) * | 2016-11-28 | 2017-06-06 | 格林美股份有限公司 | A kind of preparation method of globular powdered nickel |
| CN107030293A (en) * | 2016-11-28 | 2017-08-11 | 荆门市格林美新材料有限公司 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
| CN107649689A (en) * | 2017-11-07 | 2018-02-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN110842211A (en) * | 2019-12-17 | 2020-02-28 | 云南驰宏国际锗业有限公司 | Method for controlling particle size of superfine germanium powder |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN116511493A (en) * | 2023-04-18 | 2023-08-01 | 中机新材料研究院(郑州)有限公司 | Device and method for agglomerating air flow dispersion-ion dissociation ultrafine metal powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104646679A (en) * | 2013-11-19 | 2015-05-27 | 荆门市格林美新材料有限公司 | Method for manufacturing spherical Fe-Co-Ni alloy powder |
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| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN104942301A (en) * | 2015-06-19 | 2015-09-30 | 四川金广实业（集团）股份有限公司 | Technology for producing nickel raw material for stainless steel by nickelous hydroxide |
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN106799498A (en) * | 2016-11-28 | 2017-06-06 | 格林美股份有限公司 | A kind of preparation method of globular powdered nickel |
| CN107030293A (en) * | 2016-11-28 | 2017-08-11 | 荆门市格林美新材料有限公司 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
| CN107649689A (en) * | 2017-11-07 | 2018-02-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN110842211A (en) * | 2019-12-17 | 2020-02-28 | 云南驰宏国际锗业有限公司 | Method for controlling particle size of superfine germanium powder |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN116511493A (en) * | 2023-04-18 | 2023-08-01 | 中机新材料研究院(郑州)有限公司 | Device and method for agglomerating air flow dispersion-ion dissociation ultrafine metal powder |
| CN116511493B (en) * | 2023-04-18 | 2024-03-12 | 中机新材料研究院(郑州)有限公司 | Device and method for agglomerating air flow dispersion-ion dissociation ultrafine metal powder |
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